Method and apparatus for distillation of carbonaceous material



Jan; 12 .1926.- r

' I R. M. CATLIN IETHOD AND APPARATUS FOR DISTILLATIQN OF CARBONACEOUS MATERIAL 2 sheetsheet 1 "riginal Filed August 17, 1921 D/sT/LL/Iwau'f Z ONE Jan. 12 1926.

Re. 16,252 R. M. CATLIN v METHOD AND APPARATUS FOR DISTILLATION 0F CARBONACEOUS MATERIAL 2 SheetsSheet 2 Original Filed August 17. 1921 Elsi/#477011 2'0 e v F/re Zone Reissued Jan. 12, 1926.

UNITED STATES I Re. 16,252 PATENT; OFFICE.

nonnn'r OA' ELIN, or'rnaNxnm, NEW' JERSEY, ASSIGNOB, 'ro CATLIN SHALE rnonuc'rs COMPANY, on NEW YORK, N. Y., A CORPORATION or DELAWARE.

METHOD AND APPARATUS FOR DISTILLATION OF CARBOIQTACEOUS MATERIAL.

Original No. 1,509,687, dated September'23, 1924, Serial No. 492,885, filed August 17, 1821. Application for reisanefiled- July 18, 1925. Serial No. 44,606.

To all whom it may concern:

Be it known that 1, ROBERT M. CATLIN, a citizen of the United States, residing at Franklin, county of Sussex, and State of New J ersey, have invented certain new and useful Improvements in a Method and Apparatus for Distillation of Carbonaceous Material, fully described and represented in the following specification and the accompanying drawings, forming a part of the same. a

' This invention relates to methods .of and apparatus for distillation of carbonaceous material and particularly for the distillation of shale. 1

The principal object of the invention is to provide a process by which the volatilizable-ingredients of the: carbonaceous material may be distilled oil without injurious decomposition and with the minimum amount of combustion of such ingredients, the heat for the distillation being furnished by the combustion of a. part or all of the fixed carbon remaining in the material after the volatilizable ingredients have been distilled off. The process and apparatus will be moreparticularly explained hereinafter in connection with the accompanying drawings illustrating the preferred form of apparatus embodying the invention, particularly suitable for treating shale.

In drawings: f l Figure 1 is a diagrammatic view of the Figure, 2 is a detail sectional vew, and Y Figure 3 is a diagrammatic View of a modification of the apparatus.

' Referring to the drawings, A indicates I the outer wall or shell of an apparatus resembling a gas producer, vbut embodying some special features as hereinafter described.

The inner wall or lining B of this producer is formed of suitable refractory material, such, for example, as fire brick, the interior surface of this lining l3 sloping outward and downward so as to form a chamher which in the example show-n'is frustotinuously feeding broken carbonaceous material, for example, shale, to the producer chamber without admission of air thereto, as will be more fully explained hereinafter. Also there is provided a special means for leading off or withdrawing gases and vapors from the top of the producer chamber, and means for removing the solids from the bottom of the producer chamber at any desired or required intervals, also without any appreclable admission of air..

For the combustion of the fixed carbon'an air-gas mixture is supplied to the producer chamber by controllable means whereby the composltion of the said mixture, both as to quality and proportions, may be regulated.

The means for removing the solids from the bottom of the producer chamber comprises a suitable shaking grate located-at the bottom of the producer chamber and arranged to be operated'from the exterior of the'producer in any suitable way. This grate is indicated at D and as shown comprises 'a plurality of rocking grate bars d through the grate. This ash pit F may have a hopper bottom, as shown, with a dischargeopening 7 arranged to be controlled by a suitable gate-mechanism, which in the example --illustrated is a sliding or swinging gate f. When this gate is slid or swung back the ashes will be discharged from the ashpit. By the use of a gate such as shown it is possible to closethe discharge opening v before all the solids are discharged from the ash-pit, thus retaining some of the solids to serve as a seal against the admission of air to the producer through the discharge 7 opening. closed quickly and immediately after the discharge of all the solids from the ashpit, the amount of air admitted durin the emptying of this ash-pit may be ren ered negligible. 7

At the ash-pit, at a place above the" high- However, as the gate maybe est level to which the ashes or solids are per mitted to accumulate, there are arranged suitable blast inlets for the air mixture. In the example illustrated in the drawings, the gas and air are introduced separately to the plenum or space below the grates, as, for example, by providing concentrically arran ed pipes for air and gas, as indicated in ig. 2, and more fully described hereinafter. This avoids the possibilitv'of forming an explosive mix ure in the pipes themselves. I y

The means for feeding the broken shale or similar material to the producer chamber comprises a large magazine mounted upon the producer, as indicated at H. This maga zine is advantageously proportioned so as to hold enough material for'a run of 24 hours or longer. It has a conical or hopper-like bottom, as shown, the opening in the bottom having a diameter substantiallythe same asthe topof-the prothe inner diameter of ducer chamber.

The top of the magazine may be asdesired, but preferably is conical asshow'n, and

is provided with a dome h, closed at the top by-a suitable closure device, such, for example, as the sliding gate h or hinged door sealed with clay. a

For the purpose of continuously leading oil the gases and vapors from the produced chamber, and at the same time not interfering with the continuous feed of the brokenshale or other similar material to said chainber, there is provided a hell I, of conical form, having a bottom openin of such diameter as to cover an appreciab e part of the upper end of the producer chamber. In the example shown the diameter of the bell opening is more than half the diameter of the upper end of the producer chamber. The upper or outer surfaceof the bell forms a deflector to direct the material radially outward as it moves downward in the mega zine H, thereby causing 'it to fall in an outward direction as it enters the upper end of the. producer chamber. But since the hopper bottom of the magazine forces the material to discharge radially inward and discharges more material than does the bell,

the resultant efl'ect is to throw-the coarser material more toward the center of the producer chamber. Since the lar er pieces have a greater tendency to slide (gown/the slope than the smaller pieces, they go further toward the center of the producer than the smaller ones, with the result that the center of the producer is chargedwith the larger lumps and the wall-portion of the charge is mostly made up of smaller lumps. As a result the gases and vapors can escape freely to the bell, I. The bell is connected to a riser pipe I which most advantageously is carried some distance up throu h the center of the magazine so as to give 0 heat to the descendingcharge, and thenis turned outward through the wall of the magazine and is connected to a main K which leads to a condenser L.-

In the condenser L the vapors are condensed and the gases, consisting largely of nitrogen, -but also containing some other constituents, such as CO and perhaps some C0, are ,led back by a pipe M to the pro-' ducer, reaching the same through the pipes G and G, a suitab e suction being maintained by a fan M.

Means provided for mixing some air.

with the gases immediately at the respective inlets, as, for example, by providing an airsupply pipe N which conducts air from a suitable source -as,for example, a fan (not shown) to afbu'stle pipe N feeding air to nozzles n, each concentrically arranged inside its nozzle of the gas-supplying system, as shown in Fig.2.

The pipes M, N and G are provided with control valves as indicated at n and 9, respectively. By means ,of these valves it is possible to controlthe proportions and total amount of air-gas mixture supplied to the producer. 7

In carrying out my process the producer is so run that an ash bed or zone is maintained just above the grate, as indicated in the drawings. Above this is 'a zone of combustion in which the fixed carbon of the shale or 1 other carbonaceous material is burnt either .wholly or to any lesser extent as may be desired. Generally it is unnecessaryto burn all the fixed carbon from the material, since sufiicient heat is obtained without the complete combustion of the carbon. The zone of combustion will be referred to hereinafter as the fire zone. Above it is the 'zone of distillation wherein all the volatile products of the carbonaceous material are distilled off by hot gases coming from the fire zone.

The downward travel of the material is controlled by the amount of ashes shaken through the grate, which'of course do ends upon the frequency of operation 0 the shaking mechanism. The relative depth of the ash zone also is determined by the shaking and by the rapidity of combustion.

The depth of the fire zone is determined by the rapidity of combustion, Which can 'be regulated by the control of the supply of rial, containing fixed carbon but no volatile hydrocarbons, between the lower part of the controlled bya valves.

In the best operation of the apparatus a temperature of between 750 and 850 F, should be maintained in a zone terminating above the top of the fire zone, while the rate of downward movement of the material may well be such that it would take not less than about one hour and twenty minutes for the material to pass through this zone of approximately 800 F.

It is to be noted that the air-gas mixture enough,air to bring about the combustion in the fire zone ofthe desired amountof fixed carbon, while the volume of diluting or inert gas shouldbe enough to transport heat fromfth'e fire zone to the distillation zone so as to distill off all the volatilizable hydrocarbons and compounds at a place above the top of the fire zone.

.Since any CO in the diluent gases fed in with the air may be decomposed to CO by contact with incandescent carbon, it may be necessary, if the proportion of the CO in the gases coming from the condenser is relativel high, to burn the CO to CO before intro ucing the air-gas mixture to the producer. '-This may be done by running the gases from the condenser through a furnace withsome air. [The resulting burnt gases may'then be led to the producer. This will be clear from Fig. 3, which shows the same apparatus as in Fig. 1, with a furnace ini the terpolated between the condenser and the gas producer. The furnaceris indicated diagrammatically only at L with the pipe M leading from the condenser to it, and with the ipe M", fan'M and pipe G for taking burnt gases from the furnace to the gas producer. I

Since the continuous supply of air to the apparatus and the combustion of the oxygen of such air will provide a surplus of nitrogen and CO itwill be necessary to vent some of the gases at intervals from the system. In order to do this, a vent pipe P is providedfat any suitable point. In the best embodiment of the system, the vent pipe islocated at the upper end of the receptacle so that the hot gases will pass ofi through the broken material in the recep tacle, thus serving to dryand preheat the material. What I claim is: 1. Theprocess of distilling carbonaceous material containingv a volatilizable ortion and a combustible solid portion, whidli comprises feeding such material in a descending column, maintaining a zone of combustion at the lower part of the column by supplying a reformed inconibustible mixture oi air ant incombustible gas to the lower part of said combustion zone, regulating the quantity of said air-gas mixture to maintain a distillation zone above, the combustion zone, regulating the proportions of said airgas mixture to prevent combustion in said distillation zone, leading oii' the evolved gases and vapors from the-column above the distillation zone, separately obtaining, froni' said evolved-gases and vapors, the condensible portions thereof and also a supply of incombustible gas, and using-said incombustible gas to form the i'ncombustible air-gas mixture for subsequent distillation of carbonaceous material such as described. should have enough, but no more than" 2. The process of distilling carbonaceous .material containing volatile material and a combustible solid, which consists in feedbustion zone, regulating the amount of the air-gas mixture to maintain a distillation zone above the combustion zone and regulating the proportions of said mixture ,to prevent combustion in the distillation zone, leading off the gases and other volatilizable products from the upper part of the column. condensing the vapors from such volatilizable products and gases, burning the gases to render inert-any non-inert products in in said gases, and using the burnt gases as a diluent for making the air-gas mixture supplied to the combustion zone.

v 3. The process of distilling carbonaceous material containing volatile material and a combustible solid, which consists in feedingsuch' material in a descending column while maintaining a zone of combustion at the lower part of the column by supplying a preformed mixture of air diluted with .inert gases, to the lower part of said combus tion zone, regulating the amount of the airgas mixture to maintain a distillation zone nets and gases, burning the gases to convert any CO'to CO and usingthe burnt 'gases as a diluent for making the air-gas mixture supplied to the combustion zone.

4. The process of distilling shale containing a volatilizable portion and a combustible solid portion, which comprises feeding the shale in a descending column, maintaining a zone of combustion at the lower part lab incombustible mixture of air-and incombustible gas to the lower part of said combostion zone,'regul ating the quantity and proportions of said air-gas mixture to main tain a distillation zone above the combustion zone while preventing combustion in said distillation zone, leading off evolved gases and vapors, and condensing a liquid hydrocarbon product therefrom. I

5. In an apparatus for distilling carbonaceous material, the combination with a gas producer. having its walls sloping downwardly and outwardly, and a magazine for the material above the gas producer and having a hopper shaped bottom opening into the top of the gas producer, of a bell for leading oil gases and vapors, said bell having an outward and downwardly sloping surface, said bell being located within the ma azine and having its lower edge about in t e same plane asthe edge of the hopper opening, the diameter of the bell in said plane being such as to leave a space for the downward feed of material from the magazine to the gas pipe connected to the bel 6. In an apparatus for distilling carbonaceous material containing volatilefma-terial and a combustible residue, the combination, with a as producer having a'shaking grate, a closedash-pit beneath the grate, and a magazine for lumps. of, material above the gas producer and arranged to feed thereto the carbonaceous material to be distilled, said magazine having a charging opening with a closure therefor, of means at the upper part of the gas producer for leading off gases and vapors, a conduit for supplying compressed air to the gas producer beneath the grate thereof, means for. controlling the conduit toregulate the amount of air supplied, controllable means for directing inert gas below the grate at the point of entrance of the compressed air to form a preformed mixture of air and inert gas, and a source of inert gas supply connected to said controllable means.

7. In an apparatus for distilling carbonaceous material containing volatile material and a combustible I'GSltlllE', the combination,

. with a (gas producer having a shaking grate, a close ash-pitlocated beneath the grate,

and a magazine for lumpsof material above the gas producer and arranged to feed there to the carbonaceous material to be distilled,

said magazine having a charging opening wlth a clwure therefor, of means at the upper part of the gas producer for leading off producer, and a discharge gases and vapors, a condenser in communication with said means, a furnace into which gases pass from said condenser, means for conducting inert gases from said furnace beneath the grate, a conduit for supplying air beneath the grate. in close proximity to the point of entrance of the inert gases to insure a mixing of the air and inert gas, and means for separately regulating the air and gas supply to control the proportions of the mixture and the rate of admission thereof to the gas producer.

8.,In an apparatus 'for distilling carbonaceous material containing volatile material and a combustible residue, the combination, with a gas p .oducer having a shaking grate,

a closed ash-pit located beneath the grate,

and a magazine for lumps of material above the gas producer and arranged to feed thereto the carbonaceous material to be distilled, said magazine having a charging o e-ning with a closure therefor, of means at t pcr part of the gas producer for leading off gases and vapors, a condenser in communication with said means, means for conduct- 1ng inert gases only from said condenser beneath the grate, a conduit for supplying air 'beneath the grate in close proximity to the point of entrance of the inert gases to ine up-' sure a mixing of the air and inert gas, means i for'separately regulating the air and s supply" to control the proportions of the IIllX- ture and the rate of admission thereof to the gas producer, and means for conducti away surplus gases from the top of the magazine. 1

9. In an apparatus for distilling carbonaceous material, the combination, with a. gas producer having a shaking grate, a closed ash-pit beneath the grate, arranged to pro-- Wide a distributing space between the grate and the ashes, and a magazine for lumps of material above the gas producer and arranged to feed said material thereto, Said magazine having a charging opening with a closure, of means at the upper part of the gas producer for leading off gases and vapors, a condenser in communication with said means and arranged to condense the vapors, a furnace into which .gases pass from said condenser, means for conducting inert gases from said furnace" to the distributing space of the ash-pit, means for admit ting air with said gases and means for separately regulating the admission of air and of gas to control the proportions of the mixture and the rate of admission thereof to the ROBERT M. 'CATLIN.

gas producer. 

